CN115196686A - Method for large-scale preparation of high-purity iron oxide red - Google Patents
Method for large-scale preparation of high-purity iron oxide red Download PDFInfo
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- CN115196686A CN115196686A CN202211019374.9A CN202211019374A CN115196686A CN 115196686 A CN115196686 A CN 115196686A CN 202211019374 A CN202211019374 A CN 202211019374A CN 115196686 A CN115196686 A CN 115196686A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 102
- 229910052742 iron Inorganic materials 0.000 claims abstract description 50
- 239000012141 concentrate Substances 0.000 claims abstract description 44
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 239000002002 slurry Substances 0.000 claims abstract description 14
- 238000011031 large-scale manufacturing process Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 230000018044 dehydration Effects 0.000 claims abstract description 8
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000004806 packaging method and process Methods 0.000 claims abstract description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 56
- 229910001566 austenite Inorganic materials 0.000 claims description 6
- 229910000859 α-Fe Inorganic materials 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 229960005191 ferric oxide Drugs 0.000 description 49
- 238000007254 oxidation reaction Methods 0.000 description 18
- 230000003647 oxidation Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- 230000008901 benefit Effects 0.000 description 7
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 4
- 229910001448 ferrous ion Inorganic materials 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical group O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for preparing high-purity iron oxide red in a large scale, relates to the technical field of mineral processing, and aims to solve the problem that the existing method for producing high-purity iron oxide red by super iron ore concentrate is not suitable for industrial large-scale production; the method comprises the steps of pressing the super iron ore concentrate slurry serving as a raw material into a blank body for preliminary dehydration; placing the green body in a refractory box, and roasting in a high-temperature sintering kiln at 300-400 ℃ for 4-8h in two stages; the temperature of the second stage is 700-850 ℃, and the roasting time is 2-6h; taking out the sintered material after roasting is finished, and crushing and packaging the agglomerated iron oxide red to obtain a high-purity iron oxide red product; the method simplifies the operation steps, has simple and easily controlled process, and the prepared iron oxide red has high purity, excellent quality, small fluctuation range and good product consistency, and is beneficial to realizing large-scale production.
Description
Technical Field
The invention relates to the technical field of mineral processing, in particular to a method for preparing high-purity iron oxide red in a large scale.
Background
One of the main sources of iron oxide red raw materials used by domestic manufacturers at present is the byproduct acid-washing iron oxide red of the regeneration procedure in the cold rolling and acid-washing stage of steel. Due to the technological change of steel mills and the complicated international situation, the high-quality iron oxide red on the market is reduced, the price of the iron oxide red raw material is greatly increased, and particularly, the high-purity iron oxide red is doubled from 1500 yuan/ton to more than 3000 yuan/ton. The search for new iron oxide red sources is a critical need of many manufacturers of magnetic materials. The main component of the super iron ore concentrate is high-purity Fe 3 O 4 The method has the advantages of wide distribution, large resource quantity, high total iron content, high purity, less impurities and stable composition, and is an ideal raw material for preparing the iron oxide red.
The national patent CN1609003A discloses a method for producing iron oxide red by using iron concentrate powder, but the method has complex flow, large process control amount and many related industrial devices. Because the super iron ore concentrate after magnetic separation is in a slurry state, the super iron ore concentrate cannot be directly sent into a high-temperature kiln for oxidation. The patent adopts a method of firstly dehydrating at high temperature and then sintering and oxidizing, and iron ore concentrate is heated twice, so that energy waste is caused, and the method has no advantage in cost. And the purity of the produced iron oxide red cannot be guaranteed, and a high-purity iron oxide red raw material required by a high-end product cannot be produced in a large scale, so that good economic benefit cannot be obtained.
I have studied the preparation of high-performance permanent magnetic ferrite by taking iron ore concentrate as a raw material from 2019, and have disclosed the method for preparing high-purity iron oxide red by oxidizing super iron ore concentrate as a raw material in a muffle furnace in a laboratory lab, wherein the publication number is CN110436528A, which is named as the invention patent application of the preparation method of the high-purity iron oxide red for 9-series ferrite, mainly adopts two-stage roasting of super iron ore concentrate tiling. Therefore, a method for preparing high-purity iron oxide red on a large scale is needed to solve the problem.
Disclosure of Invention
The invention aims to provide a method for preparing high-purity iron oxide red in a large scale so as to solve the problem that the existing method for producing high-purity iron oxide red by super iron ore concentrate is not suitable for industrial large-scale production.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing high-purity iron oxide red in a large scale comprises the following specific steps:
step one, pressing the raw material into a blank for preliminary dehydration by taking super iron ore concentrate slurry as the raw material;
placing the green body in a refractory box, and roasting in a high-temperature sintering kiln at two stages, wherein the temperature of one stage is 300-400 ℃, and the roasting time is 4-8h; the temperature of the second stage is 700-850 ℃, and the roasting time is 2-6h;
and step three, taking out the sintered material after roasting is finished, and packaging the agglomerated iron oxide red after crushing to obtain a high-purity iron oxide red product.
Preferably, the total iron content of the super iron concentrate in the feed material is greater than 71.5%.
Preferably, the raw materials are pressed into a loose blank body, an industrial press is adopted for pressing, and the pressing pressure is 8-14MPa.
Preferably, the high-temperature sintering kiln is a pushed slab kiln or a roller kiln, and deep dehydration is performed while one-stage roasting is performed.
Preferably, the super iron ore concentrate is primarily oxidized into gamma-Fe after one-stage roasting 2 O 3 Two-stage roasted gamma-Fe 2 O 3 Conversion of crystalline form to alpha-Fe 2 O 3 。
Preferably, the crushing method is to use a jaw crusher to perform coarse crushing and then use ball milling for fine grinding.
Preferably, the content of the iron oxide in the high-purity iron oxide red product is not less than 99.3%.
Preferably, the fluctuation range of the content of the ferric oxide in the high-purity ferric oxide red product is less than 0.5 percent.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for preparing the high-purity iron oxide red on a large scale directly takes the super iron ore concentrate slurry as a raw material, adopts a method of roasting after pressing, obtains a product at one time, realizes preliminary dehydration and deep dehydration in the processes of pressing and roasting respectively, simplifies the operation steps, has simple and easily controlled process, and is beneficial to realizing large-scale production.
2. The method for preparing the high-purity iron oxide red on a large scale has the advantages that the purity of the prepared iron oxide red is not lower than 99.3 percent, the quality is excellent, the fluctuation range is small, the product consistency is good, a new effective source is developed for the raw materials of the domestic industrial iron oxide red, and the method has important significance for industries such as magnetic materials and the like.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
As shown in fig. 1, a method for large-scale preparation of high-purity iron oxide red comprises the following specific steps:
step one, super iron ore concentrate slurry is used as a raw material, and in order to ensure the purity and consistency of products, the total iron content of super iron ore concentrate in the raw material is preferably more than 71.5%; pressing the raw materials into a blank and preliminarily dehydrating; preferably, the raw materials are pressed into a loose blank, the pressing can be carried out by a common industrial press, and the pressing pressure is preferably 8-14MPa;
placing the green body in a refractory box, and sending the green body into a high-temperature sintering kiln (a pushed slab kiln or a roller kiln) for roasting in two stages, wherein the temperature of one stage is 300-400 ℃, the roasting time is 4-8h, the deep dehydration function can be realized while the roasting in one stage, and the process steps are also optimized; the temperature of the second stage is 700-850 ℃, and the roasting time is 2-6h; the super iron ore concentrate is primarily oxidized into gamma-Fe after one-stage roasting 2 O 3 Two-stage roasted gamma-Fe 2 O 3 Conversion of crystalline form to alpha-Fe 2 O 3 。
Step three, taking out the sintering material after roasting is finished, crushing the agglomerated iron oxide red and then packaging to obtain a high-purity iron oxide red product, wherein in the product prepared by the method, the content of iron oxide is not lower than 99.3%, and the fluctuation range is less than 0.5%; optionally, the crushing method comprises coarse crushing by a jaw crusher and fine grinding by ball milling.
The raw materials adopted in the following examples are iron ore concentrates produced by Anhui Jinan mining company Limited, the mineral separation process is completed by medium-grade steel Tianyuan company Limited, and the specific components of the screened super iron ore concentrates are shown in Table 1.
TABLE 1 main constituents of super iron concentrate
| TFe | SiO 2 | Al 2 O 3 | CaO | MgO | TiO 2 |
| 71.88 | 0.199 | 0.328 | 0.042 | 0.051 | 0.076 |
Example 1
Taking 1000kg of super iron ore concentrate slurry (containing about 23 percent of water), dehydrating and pressing the super iron ore concentrate slurry into a blank in a press under the pressure of 8Mpa, placing the blank in a refractory box, standing the blank with enough gaps between the blanks to ensure that the blank can fully contact with air to carry out oxidation reaction, and sending the blank into a pushed slab kiln to be heated, roasted and oxidized. Setting a temperature zone, wherein the first-stage roasting temperature of the super iron ore concentrate is 300 ℃, the oxidation time is 8 hours, the second-stage roasting temperature is 850 ℃, the oxidation time is 2 hours, and after the roasting and oxidation are finished, the agglomerated iron oxide red is crushed and then packaged to obtain 750kg of high-purity iron oxide red product.
Example 2
1000kg of super iron ore concentrate slurry (with water content of about 23%) is taken, the super iron ore concentrate slurry is dehydrated and pressed into a green body in a press under the pressure of 12Mpa, the green body is placed in a fire-resistant box, enough gaps are reserved between the green body and the fire-resistant box in a standing mode to ensure that the green body can be in full contact with air to carry out oxidation reaction, and the green body is sent into a push plate kiln to be heated, roasted and oxidized. And setting a temperature zone, wherein the first-stage roasting temperature of the super iron ore concentrate is 350 ℃, the oxidation time is 6 hours, the second-stage roasting temperature is 700 ℃, the oxidation time is 4 hours, and after roasting and oxidation are finished, the caked iron oxide red is crushed and then packaged to obtain 742kg of high-purity iron oxide red product.
Example 3
Taking 1000kg of super iron ore concentrate slurry (containing about 23 percent of water), dehydrating and pressing the super iron ore concentrate slurry into a blank in a press under the pressure of 14Mpa, placing the blank in a refractory box, standing the blank with enough gaps between the blanks to ensure that the blank can fully contact with air to carry out oxidation reaction, and sending the blank into a pushed slab kiln to be heated, roasted and oxidized. Setting a temperature zone, wherein the first-stage roasting temperature of the super iron ore concentrate is 400 ℃, the oxidation time is 4 hours, the second-stage roasting temperature is 800 ℃, the oxidation time is 6 hours, and after the roasting and oxidation are finished, the agglomerated iron oxide red is crushed and then packaged to obtain 751kg of high-purity iron oxide red product.
Example 4
Taking 1000kg of super iron ore concentrate slurry (containing about 23 percent of water), dehydrating and pressing the super iron ore concentrate slurry into a blank in a press under the pressure of 8Mpa, placing the blank in a refractory box, standing the blank with enough gaps between the blanks to ensure that the blank can fully contact with air to carry out oxidation reaction, and sending the blank into a pushed slab kiln to be heated, roasted and oxidized. Setting a temperature zone, wherein the first-stage roasting temperature of the super iron ore concentrate is 350 ℃, the oxidation time is 6 hours, the second-stage roasting temperature is 750 ℃, the oxidation time is 3 hours, and after the roasting and oxidation are finished, the agglomerated iron oxide red is crushed and then packaged to obtain 749kg of high-purity iron oxide red product.
The main component of the super iron ore concentrate is ferroferric oxide containing about 24% of ferrous ions, and the process of preparing iron oxide red from the super iron ore concentrate is a process of oxidizing the ferrous ions in the super iron ore concentrate into ferric ions. In the test, the oxidation degree of the super iron ore concentrate is judged by detecting the content of ferrous ions in the iron oxide red. The main components of the iron oxide red are detected and shown in the table 2.
TABLE 2 example preparation of iron oxide red main component from super iron concentrate
| TFe | SiO 2 | Al 2 O 3 | CaO | MgO | TiO 2 | C(Fe 2+ ) | |
| Example 1 | 69.45 | 0.19 | 0.273 | 0.04 | 0.043 | 0.081 | 0 |
| Example 2 | 69.46 | 0.239 | 0.352 | 0.045 | 0.053 | 0.075 | 0 |
| Example 3 | 69.45 | 0.235 | 0.321 | 0.042 | 0.055 | 0.072 | 0 |
| Example 4 | 69.47 | 0.224 | 0.304 | 0.04 | 0.05 | 0.079 | 0 |
As can be seen from table 2, in each example using the technical scheme of the present invention, the iron red prepared by dehydrating, briquetting, roasting, oxidizing and crushing the super iron concentrate as the raw material has a content of ferrous ions of 0, which indicates that the super iron concentrate is sufficiently oxidized into iron red. The total iron content of the iron oxide red is over 69.45 percent, and the content of the iron oxide in the iron oxide red reaches over 99.3 percent.
In addition, the invention also carries out a large number of tests, wherein the tests comprise that super iron ore concentrate raw materials with different total iron contents of about 72 percent are adopted, different presses and high-temperature sintering kilns are adopted, different heating rates are adopted, and the like, the method has no great influence, and the content of the ferric oxide in products with various test results meets the numerical value, and has the advantage that the content fluctuation range is less than 0.5 percent.
The method provided by the invention has the advantages of simple process and short flow, can be used for large-scale industrial production, and generates good economic benefit. Provides a new effective source for the high-purity iron oxide red raw material required by high-end products.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (8)
1. A method for preparing high-purity iron oxide red in a large scale is characterized by comprising the following specific steps:
step one, pressing the raw material into a blank for preliminary dehydration by taking the super iron ore concentrate slurry as the raw material;
placing the green body in a refractory box, and sending the green body into a high-temperature sintering kiln to be roasted in two stages, wherein the temperature of one stage is 300-400 ℃, and the roasting time is 4-8h; the temperature of the second stage is 700-850 ℃, and the roasting time is 2-6h;
and step three, taking out the sintered material after roasting is finished, and packaging the agglomerated iron oxide red after crushing to obtain a high-purity iron oxide red product.
2. The method for large-scale production of high-purity red iron oxide according to claim 1, wherein: in the raw materials, the total iron content of the super iron ore concentrate is more than 71.5 percent.
3. The method of claim 1, wherein the step of preparing high purity red iron oxide on a large scale comprises: the raw materials are pressed into loose blanks, an industrial press is adopted for pressing, and the pressing pressure is 8-14MPa.
4. The method of claim 1, wherein the step of preparing high purity red iron oxide on a large scale comprises: the high-temperature sintering kiln is a pushed slab kiln or a roller kiln, and deep dehydration is performed while one-stage roasting is performed.
5. The method for large-scale production of high-purity red iron oxide according to claim 1, wherein: the super iron ore concentrate after the one-stage roasting is primarily oxidized into gamma-Fe 2 O 3 Two stage roasted gamma-Fe 2 O 3 Conversion of crystalline form to alpha-Fe 2 O 3 。
6. The method for large-scale production of high-purity red iron oxide according to claim 1, wherein: the crushing method is to use a jaw crusher to perform coarse crushing and then use ball milling to perform fine grinding.
7. The method for large-scale production of high-purity red iron oxide according to claim 1, wherein: in the high-purity iron oxide red product, the content of iron oxide is not less than 99.3%.
8. The method for large-scale production of high-purity red iron oxide according to claim 1, wherein: in the high-purity iron oxide red product, the fluctuation range of the content of iron oxide is less than 0.5 percent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282190A (en) * | 2023-01-19 | 2023-06-23 | 华北理工大学 | Low-chloride ferric oxide for sodium ion battery, preparation method and positive electrode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057277A (en) * | 1990-06-11 | 1991-12-25 | 宣化县氧化铁颜料厂 | A kind of production method of ferric oxide red colorant |
| US5376162A (en) * | 1992-01-09 | 1994-12-27 | Virgin Metals (Canada) Limited | Autogenous roasting of iron ore |
| CN1129673A (en) * | 1995-11-23 | 1996-08-28 | 黑龙江省呼中***林机修配厂 | Process for producing high grade iron oxide red from limonite |
| CN101774647A (en) * | 2010-01-08 | 2010-07-14 | 湖南有色金属研究院 | Method for producing iron oxide red pigment with ferruginous materials |
| CN109776088A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method of Strontium ferrite powder |
| CN110436528A (en) * | 2019-09-23 | 2019-11-12 | 中钢集团安徽天源科技股份有限公司 | A kind of preparation method of 9 based ferrite high-purity iron oxide red |
-
2022
- 2022-08-24 CN CN202211019374.9A patent/CN115196686A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057277A (en) * | 1990-06-11 | 1991-12-25 | 宣化县氧化铁颜料厂 | A kind of production method of ferric oxide red colorant |
| US5376162A (en) * | 1992-01-09 | 1994-12-27 | Virgin Metals (Canada) Limited | Autogenous roasting of iron ore |
| CN1129673A (en) * | 1995-11-23 | 1996-08-28 | 黑龙江省呼中***林机修配厂 | Process for producing high grade iron oxide red from limonite |
| CN101774647A (en) * | 2010-01-08 | 2010-07-14 | 湖南有色金属研究院 | Method for producing iron oxide red pigment with ferruginous materials |
| CN109776088A (en) * | 2019-04-01 | 2019-05-21 | 中钢集团南京新材料研究院有限公司 | A kind of preparation method of Strontium ferrite powder |
| CN110436528A (en) * | 2019-09-23 | 2019-11-12 | 中钢集团安徽天源科技股份有限公司 | A kind of preparation method of 9 based ferrite high-purity iron oxide red |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282190A (en) * | 2023-01-19 | 2023-06-23 | 华北理工大学 | Low-chloride ferric oxide for sodium ion battery, preparation method and positive electrode material |
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